Sulfur tetrafluoride synthesis method and reaction system

A technology of sulfur tetrafluoride and a synthesis method, applied in the chemical industry, can solve the problems such as hindering the development and growth of the sulfur tetrafluoride industrial chain, the reaction efficiency needs to be improved, and the large-scale industrial production cannot be realized.

Active Publication Date: 2021-09-07
鹤壁德瑞科技有限公司
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Problems solved by technology

However, the vigorous development of new pharmaceutical products and the electronic information industry in the past five years has caused the rapid growth of the market demand for sulfur tetrafluoride, so that the supply of this product is in short supply, and the price remains high, which hinders the further development of the downstream industrial chain of sulfur tetrafluoride.
The iodine pentafluoride method produces sulfur tetrafluoride because the reaction efficiency needs to be improved during the recycling of iodine, which forms a bottleneck of production capacity expansion and cannot realize large-scale industrial production. Therefore, it is imperative to find a new route for the synthesis of sulfur tetrafluoride with high efficiency and low cost. Provide ample material basis for the increasingly developed modern medicine and electronics industry

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  • Sulfur tetrafluoride synthesis method and reaction system

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[0035] On the one hand, the embodiment of the present application provides a synthesis method of sulfur tetrafluoride, which includes the following steps: fluorine gas and liquid sulfur undergo a gas-liquid reaction to generate sulfur tetrafluoride, the reaction pressure is 90-120KPa, and the fluorine The distance between the gas outlet and the liquid sulfur surface is 3-10mm.

[0036] In some embodiments of the present invention, in the above-mentioned synthesis method of sulfur tetrafluoride, the distance between the outlet of the fluorine gas and the liquid sulfur surface during the reaction is 3-5 mm, and the working pressure range is 99-105 KPa.

[0037] In some embodiments of the present invention, in the above-mentioned method for producing sulfur tetrafluoride, the reaction temperature is 270-320°C.

[0038] In some embodiments of the present invention, in the above-mentioned synthesis method of sulfur tetrafluoride, the reaction temperature is 280-300°C.

[0039] In ...

Embodiment 1

[0047] The purpose of this embodiment is to provide a kind of synthetic method of sulfur tetrafluoride, comprises the steps:

[0048] The fluorine gas outlet is 5mm away from the sulfur liquid surface, the liquid sulfur temperature is 290°C, the fluorine gas flux is 150 g / h, the fluorine gas is diluted with hydrogen fluoride to a volume concentration of 30%, the reactor pressure is 99KPa, at -85°C (alcohol + liquid nitrogen) Trapped in a 10-liter nickel-plated aluminum alloy gas cylinder in the cold trap 8, reacted for 6 hours, and received 2384 grams of liquefied crude product. The crude gas cylinder was heated at 40°C and 1280 grams of purified product was obtained after the spherical sodium fluoride fully adsorbed hydrogen fluoride, and the SF was detected by gas chromatography. 4 Content 86%, SF 6 8%, s 2 f 2 4%, SOF 2 0.6%, the rest is air and trace CF 4 .

Embodiment 2

[0050] The purpose of this embodiment is to provide a kind of synthetic method of sulfur tetrafluoride, comprises the steps:

[0051] The outlet of fluorine gas is 5mm away from the liquid surface of sulfur, the temperature of liquid sulfur is 300°C, the flow rate of fluorine gas is 140 g / h, diluted with hydrogen fluoride to a volume concentration of 30%, the pressure of the reactor is 110KPa, and it is placed in a cold trap 8 at -80°C (alcohol + liquid nitrogen) Trapped in a 10-liter nickel-plated aluminum alloy cylinder, reacted for 6 hours, and received 2225 grams of liquefied crude product. The crude gas cylinder was heated at 40°C and hydrogen fluoride was fully absorbed by spherical sodium fluoride, and then 1187 grams of purified product was obtained in the cold trap 8, and the SF was detected by gas chromatography. 4 Content 83%, SF 6 6%, S 2 f 2 10%, SOF 2 0.7%, the rest is air and trace CF 4 .

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Abstract

The invention provides a sulfur tetrafluoride synthesis method and a reaction system, and relates to the technical field of chemical engineering. The sulfur tetrafluoride synthesis method comprises the following steps: fluorine gas and liquid sulfur are subjected to a gas-liquid reaction to generate sulfur tetrafluoride, the reaction pressure is 90-120KPa, and the distance between an outlet of the fluorine gas and the liquid level of the liquid sulfur during the reaction is 3-10mm. The method has the advantages that by controlling the reaction temperature, the reaction pressure and the gas-liquid distance, high-quality, stable and high-yield sulfur tetrafluoride can be realized, and the benefit maximization is realized.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a synthesis method and reaction system of sulfur tetrafluoride. Background technique [0002] Sulfur tetrafluoride is an indispensable selective fluorinating agent in organic fluorine chemistry, and occupies a dominant position in the important field of fluorine chemistry, such as deoxyfluorination, in which carbonyl, hydroxyl and carboxyl groups in organic matter are converted into -CF, -CF 2 、-CF 3 With high selectivity, it can also deoxyfluorinate the acyl fluoride-COF group in organic matter into trifluoromethyl, thus establishing its special position in high-end manufacturing fields such as modern pharmaceuticals and electronic chemicals. [0003] There are at least five technical routes for the synthesis of sulfur tetrafluoride, and the most representative technical route according to the current scale of industrialization is; [0004] 1. A method for continuous...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/45
CPCC01B17/4523Y02E60/10
Inventor 马本辉冉康德冀勇
Owner 鹤壁德瑞科技有限公司
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